65 results about "Phosphorus pentachloride" patented technology

The utility model discloses an atomizing nozzle, a phosphorus pentachloride synthesis reactor and a phosphorus pentachloride synthesis system, which comprise a nozzle body, a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and an outlet, the second inlet and the fourth inlet are both used for introducing first gas, and the fifth inlet is used for introducing second gas; the atomizing nozzle disclosed by the utility model can strengthen gas-liquid mixing and control the size and the shape of atomized particles, and in addition, the atomizing nozzle disclosed by the utility model is arranged on the reactor body, so that the distribution uniformity of materials in the space of the reactor body is improved, and a high-temperature area in the reactor body is reduced or eliminated.

The invention discloses a continuous cyclic preparation method of hexafluorophosphate. The method comprises the following steps: S1, preparation of a metal salt anhydrous hydrogen fluoride solution: adding anhydrous hydrogen fluoride and metal halide salt into a reaction kettle, and uniformly mixing, so that the metal halide salt is dissolved in the anhydrous hydrogen fluoride to obtain the metal salt anhydrous hydrogen fluoride solution; s2, preparing a hexafluorophosphate anhydrous hydrogen fluoride solution: adding phosphorus pentachloride into the reaction kettle under a temperature control condition for reaction; a hexafluorophosphate anhydrous hydrogen fluoride solution is obtained; and S3, separation of hexafluorophosphate: transferring the hexafluorophosphate anhydrous hydrogen fluoride solution into a drying tower for drying, condensing gasified anhydrous hydrogen fluoride at the top of the drying tower into liquid anhydrous hydrogen fluoride by a condenser, refluxing the liquid anhydrous hydrogen fluoride into the reaction kettle in the step S1, and collecting a hexafluorophosphate product at the bottom of the drying tower. The continuous cyclic preparation method of hexafluorophosphate has the characteristics of high raw material utilization rate, simple process and good production continuity.

This invention relates to a method for preparing high-purity phosphorus pentasulfide using a low-temperature liquid phase and its application, belonging to the technical field of key materials for lithium-sulfur batteries and solid-state batteries. It solves the technical problems of high reaction temperature and high energy consumption in existing phosphorus pentasulfide preparation processes. The method includes the following steps: Step 1: Select phosphorus pentachloride, dry it, and place the treated phosphorus pentachloride in an organic solvent to form a suspension or slurry system; Step 2: Place the suspension or slurry system in a closed reactor; Step 3: Introduce a sulfur source into the reactor to allow phosphorus pentachloride to undergo a sulfidation reaction with the sulfur source; Step 4: Raise the temperature to a set point and maintain a deep sulfidation reaction to generate phosphorus pentasulfide; Step 5: After the reaction, cool, separate the solid and liquid phases, and dry to obtain the solid product of phosphorus pentasulfide. This invention features mild reaction conditions, a simplified process flow, high safety, and recyclable solvents, making it suitable for continuous and large-scale production.

The present invention provides an automatic control method for a continuous automatic production device of phosphorus pentafluoride, comprising the following steps: S10, opening the first pipeline to fill the cartridge with an inert gas, and opening the first air outlet to discharge the residual air and water vapor in the cartridge; S11, after closing the first pipeline and the first air outlet, feeding through the feed inlet, and closing the feed inlet after the feeding is completed; S12, opening the second pipeline to fill each weighing and conveying bin with an inert gas, and opening the exhaust port to discharge the residual air and water vapor in the weighing and conveying bin, and closing the second pipeline and the exhaust port; S13, opening the feed valve and the weighing and conveying unit to weigh phosphorus pentachloride and then feed it, and simultaneously opening the hydrogen fluoride supply tank to feed anhydrous HF, wherein the phosphorus pentachloride and the fluoride are fed in proportion.

The utility model discloses a phosphorus pentafluoride generating system for a lithium hexafluorophosphate generator. The phosphorus pentafluoride generating system comprises a phosphorus pentafluoride generator, a phosphorus pentachloride feeding valve, a phosphorus pentafluoride reaction valve, a phosphorus pentafluoride feeding valve and a feeding emptying valve, one end of the phosphorus pentachloride feeding valve is connected to a phosphorus pentachloride positive pressure sending tank through a pipeline, the other end of the phosphorus pentachloride feeding valve is connected to one end of the phosphorus pentafluoride reaction valve through a pipeline, and the other end of the phosphorus pentafluoride reaction valve is connected to a feeding port of the phosphorus pentafluoride generator; a discharge port of the phosphorus pentafluoride generator is respectively connected to one end of the phosphorus pentafluoride feeding valve and one end of the feeding emptying valve through pipelines, the other end of the phosphorus pentafluoride feeding valve is connected to the lithium hexafluorophosphate generator through a gas filter, and the other end of the feeding emptying valve is connected to a tail gas collecting device through a pipeline. According to the utility model, the feeding misoperation can be eliminated, the feeding safety is ensured, and the feeding can be controlled to be correct.

The present invention relates to a comprehensive treatment method for the process tail gas of lithium hexafluorophosphate, comprising the following steps: 1) absorbing the tail gas containing phosphorus fluoride and phosphorus chloride with water to obtain a mixed acid containing hydrogen chloride, hydrogen fluoride and phosphoric acid; 2) electrolyzing the mixed acid obtained in step 1) until the hydrogen chloride in the mixed acid is completely electrolyzed to obtain a solution; 3) heating the solution obtained in step 2) to cause the water and hydrofluoric acid to escape by heat, and then obtaining hydrofluoric acid after cooling. Through electrolysis and phosphorus removal treatment, fluorine, chlorine and phosphorus in the process tail gas of lithium hexafluorophosphate are fully separated, and hydrofluoric acid and chlorine are respectively prepared. The chlorine can be recycled for the preparation of phosphorus pentachloride in the production of lithium hexafluorophosphate, realizing the recycling of chlorine. At the same time, industrial-grade hydrofluoric acid can be obtained, and the added value of the product is high.

The invention relates to the technical field of phosphorus chemical industry production, and particularly discloses a production process and equipment for producing phosphorus pentafluoride, the production process comprises five steps of material preparation, feeding, fluorination reaction, condensation reflux and collection, in the material preparation stage, anhydrous hydrogen fluoride is liquefied, and the liquefaction low temperature of the anhydrous hydrogen fluoride is maintained in the whole reaction; the technical problems that in the prior art, a gas-solid reaction is used in a process for producing phosphorus pentafluoride from anhydrous hydrogen fluoride and phosphorus pentachloride, and a fluorination reaction is a strong exothermic reaction, so that temperature control is strict in the production process, and potential safety hazards exist are solved.

The invention provides a synthesis process of isophthaloyl dichloride, which comprises the following steps: firstly, adding quantitative isophthalic acid into a reaction kettle, then adding quantitative phosphorus trichloride, mixing and stirring, adding quantitative phosphorus pentachloride, then introducing chlorine, and reacting to obtain isophthaloyl dichloride. The melting point of the isophthaloyl dichloride prepared by the process is 43.2-42.8 DEG C, the purity reaches 99.95% or above, and the yield is greater than 98%. The process has the advantages of no solvent mixing, no catalyst, easily available raw materials, low cost, short reaction period, low energy consumption, high yield, convenient reactant separation and purification, simple process control, safety, reliability, high byproduct value, easy tail gas treatment and the like, and is suitable for industrial production.

The present invention belongs to the field of phosphorus pentachloride production, and specifically relates to a continuous phosphorus pentachloride preparation device, which includes a machine base and a housing assembly. The housing assembly includes a double-layer jacketed double-helix cylinder and a reaction port cylinder vertically fixed thereto. A hollow left helix assembly and a right helix assembly are provided inside the double-helix cylinder. The front ends of the two rotating main shafts are provided with heat transfer medium cavity inlets, and the rear ends are connected to solid transmission shafts. The top of the reaction port cylinder is provided with an upper end cover, and the upper end cover is provided with a phosphorus trichloride spray port and a chlorine inlet. A phosphorus trichloride spray nozzle is provided inside the reaction port cylinder. A phosphorus pentachloride discharge port is provided below the front end of the double-helix cylinder. The structure design of the fully enclosed, continuous reaction, crystallization, stirring, and pulverization integration completely changes the traditional production method of batch feeding and discharging and pouring and pulverizing. The material reaction is more sufficient, the discharge blockage is avoided, the leakage risk is reduced, the equipment has strong corrosion resistance, and the temperature and pressure regulation are more timely and accurate.

The application discloses a phosphorus pentachloride feeding station, which comprises a feeding station frame; the feeding station frame is divided into a guide rail support, a waste bag collecting chamber, a unpacking chamber and a feeding chamber; the guide rail support is located at the top of the feeding station frame and is provided with a baffle on the bottom surface; the waste bag collecting chamber, the feeding chamber and the unpacking chamber are communicated with each other and are arranged in sequence from left to right and directly below the guide rail support; the whole conveying, unpacking and waste bag collecting of the application are in a closed space, so that harmful gas generated by unpacking and feeding is prevented from being discharged outside.

The utility model discloses a kind of even feeding devices for phosphorus pentachloride production, it is related to phosphorus pentachloride production technical field, including base, the top of base both ends is fixedly connected with U-shaped support seat, the top of base one end is fixedly connected with L-shaped support plate, both ends The top of U-shaped support seat is fixedly connected with heat-insulating jacket device, the inner side wall top of heat-insulating jacket device is fixedly connected with storage bin between, the bottom output end of storage bin is fixedly connected with electric valve, the other end of electric valve is fixedly connected with buffer tank, the base provided in the utility model, on the basis of realizing heat preservation protection to avoid affecting even feeding, increase inert gas protection to avoid causing metamorphosis simultaneously, to solve the temperature of the existing phosphorus pentachloride production feeding device is difficult to control due to lack of effective heat preservation structure, and lack of inert gas protection causes security and metamorphosis problem.

The utility model discloses phosphorus pentachloride anti-caking storage equipment which comprises supporting legs and a storage tank arranged on the supporting legs, the phosphorus pentachloride anti-caking storage equipment further comprises a heat dissipation assembly arranged in the storage tank, a storage cavity and a preparation cavity are sequentially arranged in the storage tank from top to bottom, the storage cavity and the preparation cavity are communicated through a discharging pipe, and the storage cavity is communicated with the preparation cavity. A first valve is arranged on the discharging pipe, the preparation cavity is communicated with the outside through a discharging pipe, a second valve is arranged on the discharging pipe, a flow dividing pipe, a first air inlet pipe, a first exhaust pipe, a second air inlet pipe and a second exhaust pipe are arranged on the storage tank, the first air inlet pipe is arranged on the storage tank and communicated with the storage cavity, and the second air outlet pipe is arranged on the storage tank and communicated with the storage cavity. A third valve is arranged on the first air inlet pipe, and the flow dividing pipe is arranged on the first air inlet pipe. The utility model relates to the technical field of phosphorus pentachloride storage, in particular to phosphorus pentachloride anti-blocking storage equipment which is not prone to being affected with damp, facilitates heat dissipation and is better in heat dissipation effect.

The utility model relates to the technical field of phosphorus pentachloride production devices, in particular to a phosphorus pentachloride production device which comprises a reaction box and a cover body covering the upper end of the reaction box, a stirring assembly is arranged on the cover body, and a filtering unit is arranged at the upper end of the cover body. The filtering unit comprises a shell and a Z-shaped plate, the shell is fixedly connected with the cover body, the Z-shaped plate is fixed with the shell through a fixing assembly, and a chlorine supply assembly is arranged on the lower side of the reaction box. Meanwhile, chlorine is continuously conveyed into the reaction box through the chlorine supply assembly and filtered through the filtering unit, a Z-shaped plate sealing structure is adopted, when activated carbon in a filtering frame is replaced, the lower side plate face of a Z-shaped plate can automatically seal the reaction box, chlorine leakage is effectively prevented, and the safety and operation convenience of the device are remarkably improved.

The invention discloses phosphorus pentachloride production equipment and a production process thereof, and relates to the technical field of phosphorus pentachloride production.The phosphorus pentachloride production equipment comprises a reaction kettle, an air supply device and a liquid storage tank are arranged on the outer side of the reaction kettle, a motor is fixedly connected to the bottom of the reaction kettle, and an output shaft of the motor is fixedly connected with a stirrer; according to the device, phosphorus trichloride introduced into the reaction kettle is uniformly distributed through the four nozzles which are annularly distributed, phosphorus trichloride liquid is introduced by utilizing the nozzles annularly distributed on the side wall of the inner cavity of the reaction kettle, and in the process of introducing phosphorus trichloride, the nozzles are periodically oriented in cooperation with pushing and extruding of a triggering rod on an inclined plate, so that the phosphorus trichloride is uniformly introduced into the reaction kettle; the phosphorus trichloride falls into the reaction kettle from four points, compared with single-point pipeline conveying, the problem that the concentration of the phosphorus trichloride is enriched near a conveying pipeline due to long-time single-point conveying of the phosphorus trichloride can be avoided, distribution of the phosphorus trichloride can be further enhanced in cooperation with synchronous operation of a stirrer, and the subsequent mixing effect of the phosphorus trichloride and chlorine is improved.

The utility model discloses a phosphorus pentachloride horizontal crusher, which belongs to the technical field of chemical machinery, and comprises an operation table, a horizontal linkage crushing component for carrying out horizontal double-roller crushing treatment on phosphorus pentachloride raw material solids, and an air suction sealing component for absorbing toxic gas generated by the raw materials and enhancing the sealing property, the air suction sealing assembly comprises a feeding air suction assembly and a sealing inflation assembly. The horizontal linkage smashing assembly is installed at the upper end of the operation table, the feeding air suction assemblies are installed at the upper end and the lower end of the horizontal linkage smashing assembly, and the two sealed inflation assemblies are installed at the side end of the horizontal linkage smashing assembly and distributed in a bilateral symmetry mode. In this way, the device is simple in structure and easy to implement, the smashing effect is improved, the maintenance rate of daily maintenance machines is reduced through the energy-saving machine, gas absorption and sealing protection are increased, and the quality of finished products is improved.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2-chloro-6-trichloromethylpyridine. The method comprises the following steps: by taking 6-hydroxypyridine-2-carboxylic acid as a raw material, exposing an active group through acidification hydrolysis, then taking a composite solid-phase catalyst as a catalytic chlorinating agent, enabling the activated 6-hydroxypyridine-2-carboxylic acid to react with phosphorus pentachloride, carrying out primary chlorination on hydroxyl and carboxyl to obtain chlorine and acyl chloride, and continuously chlorinating acyl chloride to form trichloromethyl, by introducing the high-selectivity composite solid-phase catalyst, the problems of low yield and low selectivity in the existing preparation process of the 2-chloro-6-trichloromethylpyridine are solved, and meanwhile, the used catalyst is simple to recover.

The invention discloses tris (trimethylsilyl) phosphate and a preparation method thereof, and belongs to the field of chemical synthesis. The invention relates to a preparation method of tris (trimethylsilyl) phosphate, in particular to a preparation method of tris (trimethylsilyl) phosphate, which comprises the following steps: hexamethyldisiloxane and phosphorus pentafluoride are subjected to heating reaction under a stirring condition to obtain tris (trimethylsilyl) phosphate, and the molar ratio of hexamethyldisiloxane to phosphorus pentafluoride is (5-10): 1. Phosphorus pentachloride is replaced with phosphorus pentafluoride, and due to the fact that fluorine atoms are small in radius and large in electronegativity, phosphorus is high in electropositivity and small in steric hindrance, phosphorus pentafluoride can react with hexamethyldisiloxane more easily, a catalyst is not needed, the cost of tris (trimethylsilyl) phosphate can be greatly reduced, and the yield of tris (trimethylsilyl) phosphate is high.

The present invention relates to processes for preparing Compound (I) or a pharmaceutically acceptable salt or solvate thereof. In particular, such processes comprise cyclodehydration of a 1,2-diacylhydrazine intermediate to form the corresponding 1,3,4-oxadiazole where the cyclodehydration agent may be N,N-dimethylsulfamoyl chloride, methyl N-(triethyIammoniumsulfonyl)carbamate, phosphorus trichloride, or phosphorus pentachloride, resulting in increased product yield and purity compared to known methods. Compound (I) and pharmaceutical compositions thereof are useful as Respiratory Syncytial Virus (RSV) inhibitors.

The invention provides a phosphorus pentafluoride gas generator which comprises a generator cylinder, a distribution disc, a first feeding port, a second feeding port, a valve assembly and a discharging port, and a containing cavity is formed in the generator cylinder; the distribution disc divides the accommodating cavity into an upper cavity body and a lower cavity body, and the distribution disc is provided with a through hole for communicating the upper cavity body with the lower cavity body; the first feeding hole is used for conveying phosphorus pentachloride solids to the lower cavity; the second feeding hole is used for conveying hydrogen fluoride liquid to the upper cavity; the valve assembly is used for opening or closing the through hole; when the through hole is opened, the hydrogen fluoride liquid in the upper cavity can enter the lower cavity through the through hole; the discharge hole is formed in the generator cylinder and is used for conveying phosphorus pentafluoride gas generated by reaction in the lower cavity to the outside of the generator cylinder. The through hole can be opened or closed through the valve assembly according to needs so as to control the intensity of the reaction, the temperature and pressure in the lower cavity are prevented from being too high, the sublimation and blockage risks of phosphorus pentachloride are reduced, and the production efficiency of phosphorus pentafluoride gas is improved.

The invention belongs to the technical field of medicines, and particularly relates to an isoflavone compound, a preparation method thereof and application of the isoflavone compound in preparation of a medicine for treating porcine epidemic diarrhea. The isoflavone compound is prepared by the following method: carrying out Friedel-Crafts acylation reaction on substituted phenylacetic acid and resorcinol under the catalytic action of boron trifluoride diethyl etherate to generate an acylated product; reacting DMF (Dimethyl Formamide) with phosphorus pentachloride to generate a Vilsmeier reagent; and carrying out condensation reaction on the acylation product and a Vilsmeier reagent to obtain the compound. In-vitro experiments prove that the isoflavone compound not only has good anti-PEDV (porcine epidemic diarrhea virus) activity, but also can remarkably relieve inflammatory response induced by PEDV. In addition, a fluorescence resonance energy transfer experiment is adopted, and it is verified that the isoflavone compound can inhibit PEDV 3C sample protease activity. The invention provides a candidate medicine for treating porcine epidemic diarrhea, and has important significance on development and innovation of isoflavone compounds.

The utility model discloses a phosphorus pentachloride tail gas treatment device which comprises a treatment box body, a gas inlet is formed in the surface of one end of the treatment box body, a gas outlet is formed in the surface of the other end of the treatment box body, filter plates are fixed in the treatment box body at equal intervals, and an electric control box is installed on the surface of one side of the treatment box body. A cleaning assembly is arranged on the top end surface of the treatment box body; through the designed cleaning assembly, dust and impurities attached to the surface of the filter plate can be conveniently cleaned, workers do not need to disassemble the filter plate for cleaning, the automation degree is high, the operation procedures of the workers are reduced, the cleaning efficiency is improved, and the practicability is good; according to the phosphorus pentachloride tail gas treatment box, through the designed functional assembly, primary filtration and adsorption treatment can be conveniently achieved when phosphorus pentachloride tail gas enters the treatment box body through the gas inlet, peculiar smells in the tail gas can be adsorbed, the follow-up treatment efficiency and effect on the phosphorus pentachloride tail gas can be conveniently improved, and the practical effect is good.

The invention discloses a preparation method of fluorophosphate, which comprises the following steps: in an organic solvent, anhydrous metaphosphate and oxalyl fluoride react to generate difluorophosphate and / or hexafluorophosphate, the structural formula of the anhydrous metaphosphate is MPO3, the structural formula of the difluorophosphate is MPO2F2, the structural formula of the hexafluorophosphate is MPF6, and in the formulas, M is selected from Li, Na or K. According to the method, high-toxicity and high-irritation raw materials such as hydrofluoric acid, phosphorus pentachloride and sulfuric acid do not need to be adopted, dangerous intermediates such as phosphorus pentafluoride and hexafluorophosphoric acid are not generated in the process, the process is simple and environmentally friendly, and the prepared fluorophosphate product is high in purity, few in impurity and suitable for lithium batteries.

The invention discloses phosphorus pentachloride production equipment and a production process thereof, relating to the technical field of phosphorus pentachloride production. The equipment comprises a reactor, wherein an air supply device and a liquid storage tank are provided on the outside of the reactor, a motor is fixedly connected to the bottom of the reactor, and an agitator is fixedly connected to the output shaft of the motor. Four nozzles arranged in an annular manner ensure that the phosphorus trichloride introduced into the reactor is evenly distributed. The device introduces phosphorus trichloride liquid by using the nozzles annularly distributed on the side wall of the inner cavity of the reactor. During the process of introducing the phosphorus trichloride, the nozzles cooperate with a trigger rod to push an inclined plate, so that the directions of the nozzles are periodically changed, so that the phosphorus trichloride falls into the interior of the reactor from four points. Compared with single-point pipeline transportation, the device can avoid the problem of phosphorus trichloride concentration enrichment near the transportation pipeline caused by long-term single-point transportation of phosphorus trichloride. Synchronous operation of the agitator can further enhance the distribution of the phosphorus trichloride and improve the subsequent mixing effect with chlorine.

The invention relates to the technical field of organic synthesis, in particular to 3-chloro-L-alanine hydrochloride and a preparation method thereof. The preparation method comprises the following steps: S1, continuously feeding a phosphorus pentachloride solution and a serine methyl ester hydrochloride solid into a dynamic tubular reactor for reaction, and carrying out solid-liquid separation, washing and drying on the reacted material to obtain 3-chloroserine methyl ester hydrochloride; and S2, mixing the 3-chloroserine methyl ester hydrochloride with hydrochloric acid, refluxing with boiling water, and drying to obtain the 3-chloro-L-alanine hydrochloride. According to the method, the reaction efficiency is greatly improved, meanwhile, the safety is good, the prepared product is high in yield and purity, and the method is suitable for industrial production.

The invention discloses a xanthene dye synthesis method, which comprises: (1) in the presence of an alkali and a catalyst, carrying out an esterification reaction on a hydroxyl group on sulfonyl fluorescein by using an esterification reagent to obtain an intermediate A; and (2) in the presence of alkali and a nickel catalyst, carrying out C-N bond coupling reaction on the intermediate A and an amine compound to obtain the target xanthene dye 2. According to the synthesis method of the xanthene dye, the situation that in a traditional synthesis method, sulfonyl fluorescein needs to be chlorinated through a strong-acidity and strong-corrosivity chlorination reagent such as phosphorus oxychloride or phosphorus pentachloride or thionyl chloride is avoided, generation of a large amount of strong-acidity gas is reduced, corrosion to production equipment is reduced, and the production cost is reduced. And the nickel-catalyzed C-N coupling reaction conditions are mild, the reaction temperature is greatly reduced, the energy consumption is reduced, and the synthesis method is more suitable for large-scale industrial production.

The invention provides a treatment method of tail gas containing phosphorus pentafluoride and a preparation method and device of lithium hexafluorophosphate. The treatment method of the tail gas containing phosphorus pentafluoride comprises the following steps: 1) carrying out first absorption treatment on the tail gas containing phosphorus pentafluoride by adopting a first absorption liquid containing lithium fluoride to obtain a first lithium hexafluorophosphate solution and a first mixed gas containing hydrogen fluoride; 2) carrying out first reaction on phosphorus pentachloride and the first mixed gas to obtain second mixed gas containing phosphorus pentafluoride; and 3) carrying out second absorption treatment on the second mixed gas by using a second absorption liquid containing lithium fluoride to obtain a second lithium hexafluorophosphate solution and a third mixed gas containing hydrogen fluoride and hydrogen chloride. According to the treatment method of the tail gas containing phosphorus pentafluoride, provided by the invention, the content of phosphorus pentafluoride in the tail gas can be reduced, and the resource utilization rate is improved.

The application relates to the technical field of phosphorus pentafluoride preparation, and provides a phosphorus pentafluoride gas generator, which comprises a generator cylinder body and a filtering structure, the generator cylinder body is internally provided with a reaction cavity, the generator cylinder body comprises an upper cylinder body and a lower cylinder body, the upper cylinder body is provided with a first feeding port for feeding phosphorus pentachloride solids into the reaction cavity, and the lower cylinder body is provided with a second feeding port for feeding hydrogen fluoride liquid into the reaction cavity; the filtering structure is arranged between the reaction cavity and the second feeding port, and is used for permeating the hydrogen fluoride liquid and blocking the phosphorus pentachloride solids. The phosphorus pentafluoride gas generator provided by the application can make the hydrogen fluoride liquid and the phosphorus pentachloride solids fully contact in the reaction cavity by arranging the filtering structure for permeating the hydrogen fluoride liquid and blocking the phosphorus pentachloride solids, so that the reaction rate is improved, and the preparation efficiency of phosphorus pentafluoride gas is improved.

The present disclosure relates to a process for the preparation of ultra high purity alkali metal hexafluorophosphate (MPF6) comprising the steps of (a) charging alkali metal fluoride (MF) into a first reactor 'B' and flushing the first reactor 'B' with nitrogen, (b) cooling the first reactor 'B' to a predetermined temperature, the method comprises the following steps: (a) dissolving an alkali metal fluoride (MF) into a first reactor 'A', then charging anhydrous hydrogen fluoride (AHF) gas into a first reactor 'B' and stirring the mixture comprising the alkali metal fluoride (MF) dissolved in the AHF, (c) cooling the mixture comprising the alkali metal fluoride (MF) dissolved in the AHF in the first reactor 'B' to a predetermined temperature, (d) charging phosphorus pentachloride (PCl5) into a second reactor 'A' and adding the AHF in batches, the invention relates to a method for producing phosphorus pentafluoride (PF5) and hydrogen chloride (HCl) gas, (e) reacting alkali metal fluoride (MF) dissolved in AHF in a first reactor 'B' with a mixture of phosphorus pentafluoride (PF5) and hydrogen chloride (HCl) gas obtained in step (d) to obtain an alkali metal hexafluorophosphate mother liquor dissolved in AHF under the coverage of PF5 gas, (f) cooling the first reactor 'B' to a predetermined temperature, and (f) separating the alkali metal hexafluorophosphate mother liquor from the first reactor 'B' to obtain the phosphorus pentafluoride (PF5) and hydrogen chloride (HCl) gas. The present invention relates to a method for preparing an alkali metal hexafluorophosphate (MPF6), characterized in that the alkali metal hexafluorophosphate (MPF6), selected from NaPF6 or KPF6 or CsPF6, is dissolved in AHF, and the alkali metal hexafluorophosphate mother liquor dissolved in AHF is maintained at said temperature for a predetermined time, followed by filtration and drying at a predetermined temperature, to obtain the alkali metal hexafluorophosphate (MPF6) selected from the group consisting of NaPF6 or KPF6 or CsPF6.

The invention discloses a synthesis method of a key intermediate 4-bromo-2-fluoro-N-methyl benzamide of an anti-prostatic cancer drug enzalutamide. According to the method, 4-bromine-2-fluorobenzaldehyde (II) is taken as an initial raw material and firstly reacts with phosphorus pentachloride, and then a compound (III) reacts with a methylamine reagent (IV) to prepare the target product 4-bromine-2-fluoro-N-methylbenzamide (I). The method disclosed by the invention has the characteristics of short steps, simple process, simplicity and convenience in operation, high total yield and the like, so that the method has relatively high implementation value and social and economic benefits.